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Polyoxymethylene dimethyl ether product system composition analysis method

A technology for polyoxymethylene dimethyl ether and composition analysis, which is applied in the field of chemical analysis, can solve the problems that analysis and detection methods cannot meet the requirements of accurately analyzing the composition of PODE product systems, and achieve good linear correlation, meet the requirements of accurate detection, reduce The effect of small errors

Pending Publication Date: 2021-08-24
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the biggest difficulty in analyzing the reaction product lies in the HF n and MG n Analysis of HF in PODE products n There are few reports on the discussion of the quantitative analysis, which leads to the inability of the existing analysis and detection methods to meet the requirements of accurate analysis of the composition of the PODE product system

Method used

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  • Polyoxymethylene dimethyl ether product system composition analysis method
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  • Polyoxymethylene dimethyl ether product system composition analysis method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] 1.1 Reagents and instruments

[0061] Methanol, methyl formate, methylal, paraformaldehyde, and ethylene glycol diethyl ether are all chromatographically pure, PODE 2 、PODE 3 Pure product (GC≥99.5%) provided for Beijing Dongfanghongsheng Research Institute; Agilent 7890B gas chromatograph, FID detector; chromatographic column: Agilent HP-1, 30m×0.320mm×0.25μm; Agilent HP6890-5973 gas phase Chromatography-mass spectrometry.

[0062] 1.2 Experimental conditions

[0063] 1.2.1 Gas chromatography analysis conditions

[0064] Agilent HP-1 capillary column (30m×0.320mm×0.25μm); column temperature adopts temperature program: 40°C for 5.0min, 50°C / min to 250°C for 5.8min; vaporization chamber temperature: 280°C; carrier gas : nitrogen, flow rate 1.0mL / min; split injection, split ratio 100:1; FID detector: 300°C, hydrogen: 30mL / min, air: 400mL / min, makeup gas: 25mL / min; sampling method: Automatic sampling; injection volume: 0.3-0.5 μL.

[0065] 1.2.2 Working conditions of ...

Embodiment 2

[0073] Embodiment 2 result and discussion

[0074] 2.1 PODE n Qualitative analysis of synthetic products

[0075] PODE n The qualitative analysis of each component in the synthetic product was mainly obtained by pure substance control and gas chromatography-mass spectrometry. like figure 1 Shown, for PODE n The gas chromatography-mass spectrogram of the synthesized product, for figure 1 The main components in the mass spectrogram analysis can determine the PODE n There are polymethoxy dimethyl ethers (PODE) with different degrees of polymerization in the product. 2-10 ), in addition, there are also unreacted raw materials and other impurity components in the product, such as DMM, TOX, HCHO, MeOH, MF, etc. Table 1 is PODE n Each component corresponds to the gas chromatography-mass spectrum retention time in the product, wherein the chromatographic peaks at 1.835min and 4.565min pass through possible reaction products and mass spectrograms (such as Figure 2-3 Shown) An...

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Abstract

The invention provides a polyoxymethylene dimethyl ether product system composition analysis method, which comprises the following steps: carrying out correction by taking ethylene glycol diethyl ether as an internal standard substance, taking a peak area ratio of methanol, methyl formate, trioxymethylene and polyoxymethylene dimethyl ether (PODEn is less than or equal to 3) to an internal standard substance as a vertical coordinate, taking a mass ratio of a compound to the internal standard substance as a horizontal coordinate, and carrying out regression to obtain a correction curve; by taking methylal, PODE2 and PODE3 as reference substances, calculating by an extrapolation method to obtain a relative mass correction factor of each component of PODE4-10; calculating the relative mass correction factor of polyoxymethylene hemiacetal (HFn) by using an effective carbon number method, and analyzing the content of polyoxymethylene glycol MGn quantitatively by using an indirect calculation method, so that the accuracy and precision of determining the composition of a polyoxymethylene dimethyl ether system synthesized from a water-containing formaldehyde raw material are remarkably improved; and the quantitative analysis requirements of polyoxymethylene dimethyl ether product system compositions with different water contents are met.

Description

technical field [0001] The present disclosure relates to the field of chemical analysis, in particular to a method for analyzing the composition of a polyoxymethylene dimethyl ether product system. Background technique [0002] With the increasing global energy crisis and environmental pollution, the development and effective utilization of oxygenated fuels as diesel additives has become a hot topic in the field of energy research. Polyoxymethylene dimethyl ether (referred to as PODE or DMM n ) is a low molecular weight acetal polymer with methyleneoxy as the main chain, and its structural formula is CH 3 (OCH 2 )nOCH 3 . When n=3~6, the average cetane number reaches over 76, the oxygen content reaches 47~50%, and the boiling point is 160~280°C, which is very similar to diesel oil in physical properties. Add 10%~15% PODE to diesel 3-6 No need to modify the fuel supply system of the diesel vehicle engine, it can significantly improve the combustion characteristics of di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 陈洪林梁琳琳雷骞吕高孟张小明洪正鹏冯孝庭
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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